Tag: M.W=200-300

In the chemical reaction process, reaction time, type of solvent, can easily affect the result of the reaction, thereby determining the yield and properties of the reaction product. An updated downstream synthesis route of 24878-25-9 as follows. Quality Control of 2,2′-Oxydianiline

A solution of 2-hydroxy-5-(thiophen-2-yl)benzaldehyde (3)(1.34 g, 2.0 mmol) in ethanol (30 mL) was added to a solution of2,20-oxydianiline (2-aminophenyl ether) (4) (0.66 g, 1.0 mmol) inethanol (20 mL) with continuous stirring, and the mixture wasrefluxed for 24 h. The completion of the reaction was monitoredthrough TLC. The reaction mixture was then cooled to room temperatureand ethanol was removed. The obtained residue waswashed with ethanol and dried at room temperature. The productwas recrystallized from the mixture of ethanol:kloroform (1:2). Theyield of orange product OPBTS was 46% (1.72 g), (m.p. 172-175 C).FTIR (KBr, cm-1) 3436.04 (nuO-H phenolic), 3268.00-3120.01 (nuAr C-H),1621.17 (nuCN), 1575.90e1489.00 (nuAr CC), 816.62 and 681.50 (nuC-SC).1H NMR (400 MHz, DMSO-d6) delta (ppm) 13.27 (s, 1H, ArO-H), 9.02(s, 1H, -CHN), 7.82 (d, 1H, J 2.4 Hz, Ar-H), 7.61 (dd, 1H, J 8.4,J 2.4 Hz, Ar-H), 7.55 (dd, 1H, J 7.4 Hz, J 1.8 Hz, Ar-H), 7.40 (dd,1H, J 5.2 Hz, J 1.2 Hz, Th-H), 7.30 (dd, 1H, J 3.6 Hz, J 1.2 Hz,Th-H), 7.26e7.23 (m, 2H, Ar-H), 7.04 (dd, 1H, J 5.2 Hz, J 3.6 Hz,Th-H), 6.94 (dd, 1H, J 8.0 Hz, J 1.6 Hz, Ar-H), 6.87 (d, 1H,J 8.8 Hz, Ar-H). 13C NMR (100 MHz, DMSO-d6) delta (ppm) 163.73,160.46,150.20,143.07,138.89,130.94,129.48,128.91,128.85,125.53,125.08, 123.03, 120.58, 119.82, 119.48, 117.92. Elemental anal. calcd.for C34H24N2O3S2: C, 71.31; H, 4.22; N, 4.89; O, 8.38; S,11.20%. FoundC, 70.86; H, 4.21; N, 4.90; S, 10.87%.

According to the analysis of related databases, 24878-25-9, the application of this compound in the production field has become more and more popular.

These common heterocyclic compound, 1663-61-2, name is (Triethoxymethyl)benzene, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. category: ethers-buliding-blocks

General procedure: The starting hydrazide 4, 8e-i (10 mmol) was added to a mixture of the appropriate triethyl orthoester (10 mol) and 0.1 g p-TsOH in 20 mL of xylene and kept under reflux for 3 h (TLC). After cooling, the mixture was washed with water (30 mL), dried over MgSO4 and then concentrated under reduced pressure. The oily residue was subjected to column chromatography (silica gel, eluent: hexane/AcOEt, 1:2 v/v) or crystallised from benzene/hexane mixture.

The synthetic route of (Triethoxymethyl)benzene has been constantly updated, and we look forward to future research findings.

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 22171-15-9, name is (4-(Benzyloxy)phenyl)methanamine, This compound has unique chemical properties. The synthetic route is as follows., Product Details of 22171-15-9

Preparation Example A+-8. N-(4-Benzyloxy-benzyl)-6-(ethoxymethyl-amino)-nicotinamide To a solution of 6-aminonicotinic acid (130mg, 0.941 mmol) and 4-benzyloxy-benzylamine (201 mg, 0.941 mmol) described in Preparation Example 1 in N,N-dimethylformamide (5mL), was added benzotriazol-1-yl-tris(dimethylamino)phosphonium hexafluorophosphate (624mg, 1.41mmol) and triethylamine (394mul, 2.82mmol), and the solution was stirred for 40 minutes at 80C. Water and ethyl acetate were added to the reaction solution, which was then partitioned, and the organic layer was washed twice with water. The solvent was evaporated in vacuo, ethyl acetate was added to the residue, a white insoluble matter was collected by filtration, and 6-amino-N-(4-benzyloxy-benzyl)-nicotinamide (202mg, 0.606mmol, 64%) was obtained. To a solution of the resulting 6-amino-N-(4-benzyloxy-benzyl)-nicotinamide (200mg, 0.556mmol) in ethanol (10mL) were added 5,5-dimethylimidazophospho-2,4-dione (85mg, 0.66mmol) and 37% formaldehyde aqueous solution (1mL), and the solution was stirred for 1 hour under reflux. Water and ethyl acetate were added to the reaction solution, which was then partitioned, and the organic layer was washed twice. NH silica gel was added to the organic layer, the solvent was evaporated in vacuo for adsorption, purification was carried out by NH silica gel column chromatography (ethyl acetate), and the title compound (95mg, 0.243mmol, 40%) was obtained as a white solid. 1H-NMR Spectrum (CDCl3) delta (ppm) :1.20 (3H, t, J=7.0Hz), 3.55 (2H, q, J=7.0Hz), 4.56 (2H, d, J=5.5Hz), 4.84 (2H, s), 5.07 (2H, s), 5.68 (1 H, brs), 6.14 (1 H, brs), 6.62 (1 H, d, J=8.8Hz), 6.96 (2H, d, J=8.8Hz), 7.22-7.35 (4H, m), 7.27-7.44 (3H, m), 7.93 (1 H, dd, J=2.4, 8.8Hz), 8.54 (1 H, d, J=2.4Hz).

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 22171-15-9.

Researchers who often do experiments know that organic synthesis is a process of preparing more complex target molecules from simple raw materials through one or more chemical reactions. Generally, it requires fewer steps, and cheap raw materials. 450-88-4, name is 1-Bromo-4-fluoro-2-methoxybenzene, A new synthetic method of this compound is introduced below., category: ethers-buliding-blocks

To a stirred solution of 1 -bromo-4-fluoro-2-methoxybenzene (4.0 g) in DMF (40 mL) was added sodium methanethiolate (2.76 g). The mixture was stirred at room temperature for 30 minutes and at 85 C for 2 h. Water was added and the mixture was extracted with ethyl acetate. The organic phase was washed with saturated sodium chloride solution, dried (sodium sulfate) and the solvent was removed in vacuum. Silica gel chromatography gave 280 mg of the title compound.1H-NMR (400MHz, DMSO-d6): delta [ppm] = 2.46 (s, 3H), 3.82 (s, 3H), 6.74 (dd, 1 H), 6.91 (d, 1 H), 7.44 (d, 1 H).

The basis of chemical reaction formula synthesis, the synthesis route is composed of some specific reactions and combined according to certain logical thinking. We look forward to the emergence of more reaction modes in the future.

These common heterocyclic compound, 5414-19-7, name is 1-Bromo-2-(2-bromoethoxy)ethane, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. Recommanded Product: 5414-19-7

TERT-BUTYL F [S- (4-BUTOXYPHENYL) thien-2-yl] sulfonyl} acetate (5) from Part C (4.0 g, MW 410.55), 18-CROWN-6 (from Aldrich, 0.5 g, catalytic amount), potassium carbonate (from Aldrich, 5.4 g, MW 138. 21,4. 0 eq), and bis (bromoethyl) ether (from Aldrich, 3.4 g, MW 231.93, 1.5 eq) were slurried in N, N-dimethylformamide (20 ML). The resulting mixture was stirred at 65C for 15 hr. Afterward, the mixture was diluted with water (50 ml) and extracted with ethyl acetate (3x-100 ml). The organics were combined and washed with water (2x), washed with brine (LX), dried over NA2S04, and concentrated for a tan oil. The oil was washed with hexanes and dried to afford tert-butyl-4-{[5-(4-butoxyphenyl) thien-2- yl] SULFONYL} TETRAHYDRO-2H-PYRAN-4-CARBOXYLATE (6) as a tan oil (4.3 g, 91 % YIELD). 1H NMR and LCMS confirmed the presence of the desired compound (6). The”equivalents” above indicate equivalents relative to the charged amount of tert-butyl {[5-(4- butoxyphenyl) thien-2-yl] sulfonyl} acetate.

The synthetic route of 1-Bromo-2-(2-bromoethoxy)ethane has been constantly updated, and we look forward to future research findings.

Some common heterocyclic compound, 332-48-9, name is 1-(2-Bromoethoxy)-4-fluorobenzene, molecular formula is C8H8BrFO, traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route. name: 1-(2-Bromoethoxy)-4-fluorobenzene

A solution of 4-methyl-2-(2H-pyrazol-3-yl)-thiazole-5-carboxylic acid benzylamide (0.2 g, 0.67 mmol) in dimethyl sulfoxide (5 mL) was treated with 4-fluorophenoxyethyl bromide (0.14 g, 0.67 mmol) and potassium carbonate (0.30 g, 2.0 mmol), and the reaction mixture was heated to 90 0C for 16 hr. The reaction mixture was cooled to room temperature, diluted with ethyl acetate (50 mL), and washed with brine (2 x 50 mL). The organic phase was dried (Na2SC^) and evaporated. The residue was purified by preparative thin layer chromatography over silica gel (methylene chloride:methanol, 95:5) to provide 2-{l-[2-(4-fluoro-phenoxy)-ethyl]-lH-pyrazol-3-yl}-4-methyl-thiazole- 5-carboxylic acid benzylamide (0.071 g, 51% yield) as a white solid.

These compound has a wide range of applications. It is believed that with the continuous development of the source of the synthetic route 332-48-9, its application will become more common.

Synthetic Route of 106854-77-7, A common heterocyclic compound, 106854-77-7, name is 1-Bromo-4-(2,2,2-trifluoroethoxy)benzene, molecular formula is C8H6BrF3O, its traditional synthetic route has been very mature, but the traditional synthetic route has various shortcomings, such as complicated route, low yield, poor purity, etc, below Introduce a new synthetic route.

Step 7: 1-Benzyl-N,4-dimethyl-N-neopentyl-3-(4-(2,2,2-trifluoroethoxy)phenyl)-5-(trifluoromethyl)-1H-pyrrole-2-carboxamide (SC-260) Under an nitrogen atmosphere 1-benzyl-N,4-dimethyl-N-neopentyl-3-(4,4,5,5-tetramethyl-1,3,2-dioxaborolan-2-yl)-5-(trifluoromethyl)-1H-pyrrole-2-carboxamide (106 mg, 0.216 mmol) was dissolved in DMF (1 mL) and LiOH (4 mg, 0.216 mmol), bis(tri-tert-butylphosphine)palladium (0) (6 mg, 0.014 mmol) and 1-bromo-4-(2,2,2-trifluoroethoxy)benzene (50 mg, 0.196 mmol) were subsequently added. The reaction mixture was stirred at 80 C. under microwave irridation for 1 h. The mixture was cooled to RT and the reaction was stopped by addition of 1M NaOH solution (2 mL). The crude product was extracted with EtOAc (2*3 mL) and the combined organic layers were washed with water (3*1 mL), dried over Na2SO4, filtered and the solvent was removed under reduced pressure. The crude mass was purified by flash chromatography to give SC-260 (95 mg, 89.7%).

The synthetic route of 106854-77-7 has been constantly updated, and we look forward to future research findings.

Each compound has different characteristics, and only by selecting the characteristics of the compound suitable for a specific situation can the compound be applied on a large scale. 1462-37-9, name is ((2-Bromoethoxy)methyl)benzene, This compound has unique chemical properties. The synthetic route is as follows., Quality Control of ((2-Bromoethoxy)methyl)benzene

EXAMPLE 17; Preparation of (5S)-N {3- [3- (2-Benzyloxy-ethoxyimino)-4- methyl-3, 4-dihydro-2H-benzo [1, 4] oxazin-7-yl)-2-oxo-oxazolidin-5-ylmethyl}- acetamide; Sodium hydride (95percent, 80 mg, 3.3 mmol) is added portionwise at 0 °C to (5S)- N [3- (3-hydroxyimino-4-methyl-3, 4-dihydro-2H-benzo [1, 4] oxazin-7-yl)-2-oxo- oxazolidin-5-ylmethyl]-acetamide (from Example 9, step 1, 0.5 g, 1.49 mmol) in DMF (15 ml). The reaction mixture is stirred at 0 °C for 30 min and then benzyl-2- bromo ethyl ether (0.360 ml, 2.27 mmol) added dropwise. The reaction is allowed to warm to room temperature and stirred overnight. The reaction is quenched with sat. ammonium chloride, diluted with ethyl acetate, washed with water and brine, dried (Na2SO4) and evaporated. The residue is purified by PTLC (10percent MeOH/DCM) to give product as a white solid (0.45 g, 64percent); HPLC r. t. 5.26 min ; 1H NMR (300 MHz, CDC13-d) 8 7.28-7. 35 (m, 5H), 7.15 (d, J = 2.4 Hz, 1H), 7.09 (dd, J = 2.4, 8. 7 Hz, 1H), 6.80 (d, J = 9 Hz, 1H), 6.10 (t, 1H), 4.98 (s, 2H), 4.76 (m, 1H), 4. 58 (s, 2H), 4.13 (m, 2H), 4.02 (t, J = 9 Hz, 1H), 3.68-3. 76 (m, 4H), 3.56-3. 63 (m, 1H), 3.22 (s, 3H), 2.03 (s, 3H); MS for C24H2sN406m/z 469.0 (M+H) +.

Chemical properties determine the actual use. Each compound has specific chemical properties and uses. We look forward to more synthetic routes in the future to expand reaction routes of 1462-37-9.

Synthetic Route of 7025-06-1, As we all know, there are many different methods for the synthesis of a compound, and people can choose the synthesis method that suits their own laboratory according to the actual situation. 7025-06-1 name is 1-Bromo-2-phenoxybenzene, This compound is widely used in many fields, so it is necessary to find a new synthetic route. The downstream synthesis method of this compound is introduced below.

1-Bromo-diphenyl ether (9.8 g, 40 mmol) was added to a three-necked flask, stirred and dissolved with 200 mL of anhydrous tetrahydrofuran, protected with nitrogen, cooled to -78 C, then slowly added dropwise 2.5 M butyl lithium 16mL of solution, stir for half an hour after addingThen, a solution of 3-bromocarbazole (9.76 g, 40 mmol) in tetrahydrofuran was added dropwise to the reaction solution, and the mixture was added dropwise to room temperature, and the reaction was stirred for 2 hours.Quenched by adding a saturated ammonium chloride solution, adding a water solution, and concentrating the organic phase.A yellow oil was obtained. The oil was added to a mixture of 100 mL of HAc and 20 mL of HCl.After cooling, the organic phase was washed three times with DCM extraction of saturated brine.The solvent was evaporated and the residue was crystallised from DCM /EtOAc.The white solid was obtained as Compound 3-1 (13.4 g, yield 82%).

At the same time, in my other blogs, there are other synthetic methods of this type of compound, 1-Bromo-2-phenoxybenzene, and friends who are interested can also refer to it.

Adding a certain compound to certain chemical reactions, such as: 75148-49-1, name is 3-Bromobenzaldehyde Diethyl Acetal, belongs to ethers-buliding-blocks compound, can increase the reaction rate and produce products with better performance than those obtained under traditional synthetic methods. Here is a downstream synthesis route of the compound 75148-49-1, Quality Control of 3-Bromobenzaldehyde Diethyl Acetal

General procedure: One equiv. of protected hydrazine was dissolved/suspended in EtOH containing 10% water (approx. 5 ml per 1 mmol of protected hydrazine), 1.05 eq of benzaldehyde acetal was added, followed by the addition of 0.05 equiv. of TsOH in an ethanolic solution (10 mg of TsOH per 0.5 ml of EtOH). The obtained reaction mixture was refluxed and monitored by TLC (silica gel) until full conversion of the starting material was observed. Ethyl acetate/light petroleum mixtures or pure ethyl acetate were used as TLC eluents. After completion of the reaction the solvent was removed under reduced pressure, approx. 15 ml of toluene was added to the residue and the solvent was again removed under reduced pressure. The obtained crude hydrazone was dissolved in commercial stabilized THF (approx. 4 ml per 1mmol of hydrazone), the flask was flushed with argon and 3 equiv. of 1M BH3-THF complex was added at room temperature, followed by 3 hours of stirring. The progress of the reaction was checked by TLC and if some unreacted hydrazone was left, stirring was continued for an additional 45 min. After thefull conversion of hydrazone EtOH (10 ml) was added to the reaction mixture (Caution: Liberation of hydrogen) and the obtained mixture was refluxed for 1 hour. After cooling to room temperature the solvent was removed under reduced pressure and the residue was dissolved in ethyl acetate, washed with saturated NaHCO3 solution, water and saturated NaCl solution. The aqueous phase was extracted twice with ethyl acetate, the extracts were washed with saturated NaCl solution, combined with the organic phase, dried over anhydrous Na2SO4 and evaporated to dryness. The residue was purified by column chromatography on silica gel by using ethyl acetate/light petroleum 1:1 or 1:2 mixtures or pure ethyl acetate as eluent. For the exact information about the eluent used for monitoring reaction progress and chromatographic purifications, see the Rf value for each compound.

In the field of chemistry, the synthetic routes of compounds are constantly being developed and updated. I will also mention this compound in other articles, 3-Bromobenzaldehyde Diethyl Acetal, other downstream synthetic routes, hurry up and to see.